石墨烯基碳纳米材料的制备及其电化学性能研究
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摘要
石墨烯，一种二维晶体结构的单碳原子层纳米材料，可称为“单层石墨片”，是碳家族中的新成员。因其集高比表面积、优异的导热导电性、优良的热稳定性及量子隧道效应等多种物理化学特性于一身，而受到人们的广泛关注，成为近十年来科学技术界争相研究的热点。碳纳米材料的性能主要取决于其本身的结构与形态，因而具有多样性特征，使得它们在储能、催化、传感器以及电子学、光学等领域展现出巨大的应用潜能。本论文的主要研究目标在于采用简单易行的物理化学法对石墨烯的结构和形貌进行处理，并系统地探讨改性后石墨烯基纳米材料的性能与结构的相互关系，研究它们在电化学电容器和锂离子电池方面的应用，取得了以下主要成果：
(1)采用一种简单而新颖的限域微观爆炸法制备出高质量的石墨烯纳米卷。该方法成功地实现了二维石墨烯向准一维石墨烯基纳米碳材料的转变，同时提出了微小气泡在超声作用下能迅速膨胀而诱导氧化石墨烯片层脱落并卷曲的形成机理。通过表征方法和电化学测试手段考察了石墨烯纳米卷的形貌结构和超电容性能。结果表明，所制备的石墨烯纳米卷具有独特的卷曲构造、两端开口和内外边缘呈开放状等结构特点，使得它具有比单一石墨烯片更优异的抗团聚性能；由于石墨烯纳米卷可利用面积大而呈现出优异的电化学电容性能，单一石墨烯的比电容仅为110F g~(-1)，而石墨烯纳米卷的电容高达162.2F g~(-1)，由此表明仅仅改变石墨烯片层的微观形貌可使其电容性能提升50%。此外，经1000次循环后，石墨烯纳米卷表现出优异的循环稳定性能。由此可知，限域微观爆炸法是一种简易制备石墨烯纳米卷的可行方法，所制备的纳米卷是一种具有广泛应用前景的新型准一维石墨烯基纳米材料。
(2)以水相Fe~(3+)离子为催化剂，采用限域微观爆炸法制备出边缘卷曲的石墨烯，与未卷曲部位构建了卷-片一体的碳纳米材料。通过透射电子显微电镜、N2吸脱附曲线和拉曼光谱研究了所制备材料的形貌和结构。结果表明，卷状结构分布在石墨烯上，形成了卷-片一体的碳纳米材料，其石墨烯的成卷率大约为30%，比表面积为251.2m2g~(-1)，该值远大于单一石墨烯(78.2m2g~(-1))的比表面积。采用循环伏安、恒流充放电以及电化学阻抗谱等电化学方法测试了所制备材料的超电容性能。结果表明，在1mol L~(-1)的硫酸溶液中，1.0A g~(-1)的电流密度下，卷-片一体碳纳米材料的比电容为224F g~(-1)，远大于单一石墨烯的137F g~(-1)和GS-MWCNTs-7-3的121F g~(-1)，由此表明卷曲形貌和卷-片一体的结构为离子或电子提供了丰富的传输通道，从而表现出良好的电解质的离子或电子传输性能以及较低的等效串联电阻，使得卷-片一体的碳纳米材料具有良好的循环稳定性能和电化学电容特性。
(3)采用强氧化-声化学切割法制备出径向长度为10-300nm、两端开口的多壁富勒烯管，并将其与石墨烯构建出复合纳米膜材料。采用扫描电子显微电镜、N2吸脱附曲线和X射线衍射光谱研究了复合膜的形貌和结构，结果表明，富勒烯管可视为一种大分子化合物用以修饰石墨烯形成多孔三维膜结构的纳米复合材料。采用循环伏安和电化学阻抗谱研究了复合膜的电化学活性，结果表明，富勒烯管的引进有效地抑制了石墨烯的团聚，促进了电子或离子在电极材料的传递速率，提高了碳纳米管管体积的利用率，因此复合膜材料呈现出很高的电化学活性。该结果为促进碳纳米管在储能方面的应用提供了有力的依据。
(4)采用具有芳香烃大分子的中间相沥青为碳源，SBA~(-1)5型有序介孔硅为模板，通过模板碳化法制备出具有纳米石墨烯片孔壁结构的多孔碳材料，探讨了该材料的形成过程和研究了其锂离子电池负极性能。采用透射电子显微电镜、N2吸脱附曲线和X射线衍射光谱等研究了多孔碳的形貌和结构。结果表明，多孔碳材料具有二维有序且对称的六边形孔结构，孔壁由纳米石墨烯片层沿垂直于孔壁轴向定向堆积而成的。经50次循环充放电后，其i0和DLi值基本保持不变，甚至在高达3500mA g~(-1)电流密度下，其可逆比容量仍具有153.9mAh g~(-1)，展现出突出的倍率性能和优异的循环稳定性能。这些优异的锂离子负极性能主要取决于多孔碳材料具有多孔性的结构和纳米石墨烯片的孔壁结构。
(5)系统探讨了热处理温度对一步浸渍-模板碳化法制备的纳米石墨烯片堆积结构多孔碳材料的锂离子电池负极性能的影响。结果表明，在1200°C (C~(-1)200)的热处理温度下制备的多孔碳材料具有纳米石墨烯片状结构的孔壁，其可逆比容量为372mAh g~(-1)；随着热处理温度的升高，达到1800°C (C~(-1)800)时，多孔碳的纳米石墨烯片状结构越清晰，锂离子电池的比容量逐渐降低，然而功率性能却与C~(-1)200相似。但是在2400°C (C-2400)的热处理温度下，多孔碳发生了重排，其孔隙壁表现为成束的无孔纳米纤维结构，表现出低的比能量-比功率性能。由此可知，热处理温度由于能影响多孔碳材料的纳米石墨烯片孔壁结构，进而能影响该材料的锂离子电池负极性能。
Graphene, a single layer of carbon atoms with two-dimensional crystal structures,is a new member of the carbon family. Graphene has attracted great attention for itsoutstanding physical and chemical properties such as high specific surface area,conductivity, thermal stability and quantum tunnel effect. In the past decade, it hasbecome a research focus. The performance of carbon nanomaterial usually depends onits structure and morphology, which show great application potential in energy storage,catalysis, sensors and electronics, optics, etc. The main targets of this paper are asfollows:(1) Graphene is modified by physicochemical methods to obtaingraphene-based nanomaterials with more excellent performances;(2) the internalconnection of structures and electrochemical properties and the electrochemicalapplications (supercapacitors and lithium ion batteries) of graphene-basednanomaterials are systematically researched, which could lay the foundation ofpractical application of graphene nanomaterials. Main research contents are as follows:
(1) High-quality graphene scrolls (GSS) are designed using a facile and novelmicroexplosion method under an ultrasonic reaction between MnO2and H2O2. Themethodology successfully realizes the transformation from2-dimensional (2D)material to nearly1D material. The scrolled mechanism is proposed and theircapacitance properties are investigated in this work. Compared with the specificcapacity of110F g~(-1)for graphene sheets, a remarkable capacity of162.2F g~(-1)isobtained at the current density of1.0A g~(-1)in6M KOH aqueous solution due to theirunique scrolled conformation, porous structure, open ends/edges and adjustableinterlayer distance. The capacity value is increased by about50%only because of thetopological change of graphene sheets. Meanwhile, GSS exhibit excellent long-termcycling stability along with96.8%retained after1000cycles at1.0A g~(-1). All datassuggest that this study could offer an insightful approach for the preparation anddevelopment of GSS. These encouraging results indicate that GSS based on thetopological structure of graphene sheets are a kind of promising material forsupercapacitors.
(2) Partial scrolled graphene are designed by a simple microexplosion techniqueusing a mild ionic catalyst-Fe~(3+), and assemble sroll-sheet conjoined nanomaterials(GS-GSS) based on graphene (GS) with unscrolled parts for enhanced supercapacitor properties. The morphology and structure of GS-GSS are characterized bytransmmision electron microscope, N2adsorption/desorption, Raman spectra andenergy dispersive spectrometer. The results demonstrate that the scrolled structurepresents on the edges of GS form GS-GSS and the scroll rate of nanomaterials is about30%. Electrochemical dates show that the specific capacitance of GS-GSS (224F g~(-1)at1.0A g~(-1)in1M H2SO4) is much higher than that of GS (137F g~(-1)) andGS-MWCNTs-7-3(121F g~(-1)), the capacity value is increased by about100%onlybecause of the difference of tubular structure (scroll has the open ends and edges,while the carbon nanotubes are closed). Therefore, the GS-GSS are promisinggraphene-based materials for supercapacitors. What's more, it is expected for GS-GSSnanomaterials to replace the traditional GS-MWCNTs nanocomposites for potentialapplications in future.
(3) In this study, for increasing the utilization of closed pore volumes of carbonnanotubes (CNTs) in conventional graphene-CNTs composites, multi-wall fullerenenanopipes (MWFNs) are adopted to replace the pristine, nearly endless and highlytangled CNTs. The CNTs are tailored into MWFNs with10-300nm lengths and openends, and a nanocomposite film of well-dispersed MWFNs as macromolecules ongraphene (GS) is prepared by a facile wet-chemical route. The morphology of theresulting materials is characterized by scanning electron microscope (SEM) and theirelectrochemical activities are investigated, suggesting that the MWFNs asmacromolecules could uniformly modify and distribute on the surface of graphene andform a film structure with graphene. The introduction of MWFNs could effectivelyenhance the utilization of closed pore volumes of nanopipes, inhibit the stacking ofgraphene and facilitate the transportation of the electrolyte ion and electron in theelectrode. Such the GS/MWFNs nanocomposites obtain ultrahigh electrochemicalactivities. These results indicate that the unique MWFNs would stimulate thedevelopment of several energy-efficient technologies.
(4) An ordered mesoporous carbon (OMC) with controllable molecule crystal andplatelet graphitic pore walls, which is directionally grown on the internal pore walls ofSBA~(-1)5or anchors at liquid/silica interfaces by molecule engineering, has beeninvestigated as lithium ion anodes. It is found that the OMC exhibits high kinetics, rateand cycling performance. The i0and DLiare almost constant after50cycles. OMCshows a high reversible specific capacity of153.9mAh g~(-1)at the current density ashigh as3500mA g~(-1). The excellent electrochemical performance could be attributed tothe presence of the porosity and platelet graphitic pore walls.
(5) Mesoporous carbons (MCs) with nanosheet-like walls have been prepared aselectrodes for lithium-ion batteries by a simple one-step infiltrating method under theaction of capillary flow. The influence of heat treatment temperature on the surfacetopography, pore/phase structure and anode performances of as-prepared materials hasbeen investigated. The results reveal that melted liquid-crystal polycyclic aromatichydrocarbons could be anchored on liquid/silica interfaces by molecule engineering.After carbonization, the nanosheets are formed as the pore walls of MCs and areperpendicular to the long axis of pores. The anode properties demonstrate that C~(-1)200displays higher reversible capacitance than those treated in higher temperature. Therate performances of C~(-1)200and C~(-1)800are similar and more excellent than that ofC-2400. These improved lithium ion anode properties could be attributed to thenanosheet-like walls of MCs which can be influenced by the heat treatmenttemperature.
(1)采用一种简单而新颖的限域微观爆炸法制备出高质量的石墨烯纳米卷。该方法成功地实现了二维石墨烯向准一维石墨烯基纳米碳材料的转变，同时提出了微小气泡在超声作用下能迅速膨胀而诱导氧化石墨烯片层脱落并卷曲的形成机理。通过表征方法和电化学测试手段考察了石墨烯纳米卷的形貌结构和超电容性能。结果表明，所制备的石墨烯纳米卷具有独特的卷曲构造、两端开口和内外边缘呈开放状等结构特点，使得它具有比单一石墨烯片更优异的抗团聚性能；由于石墨烯纳米卷可利用面积大而呈现出优异的电化学电容性能，单一石墨烯的比电容仅为110F g~(-1)，而石墨烯纳米卷的电容高达162.2F g~(-1)，由此表明仅仅改变石墨烯片层的微观形貌可使其电容性能提升50%。此外，经1000次循环后，石墨烯纳米卷表现出优异的循环稳定性能。由此可知，限域微观爆炸法是一种简易制备石墨烯纳米卷的可行方法，所制备的纳米卷是一种具有广泛应用前景的新型准一维石墨烯基纳米材料。
(2)以水相Fe~(3+)离子为催化剂，采用限域微观爆炸法制备出边缘卷曲的石墨烯，与未卷曲部位构建了卷-片一体的碳纳米材料。通过透射电子显微电镜、N2吸脱附曲线和拉曼光谱研究了所制备材料的形貌和结构。结果表明，卷状结构分布在石墨烯上，形成了卷-片一体的碳纳米材料，其石墨烯的成卷率大约为30%，比表面积为251.2m2g~(-1)，该值远大于单一石墨烯(78.2m2g~(-1))的比表面积。采用循环伏安、恒流充放电以及电化学阻抗谱等电化学方法测试了所制备材料的超电容性能。结果表明，在1mol L~(-1)的硫酸溶液中，1.0A g~(-1)的电流密度下，卷-片一体碳纳米材料的比电容为224F g~(-1)，远大于单一石墨烯的137F g~(-1)和GS-MWCNTs-7-3的121F g~(-1)，由此表明卷曲形貌和卷-片一体的结构为离子或电子提供了丰富的传输通道，从而表现出良好的电解质的离子或电子传输性能以及较低的等效串联电阻，使得卷-片一体的碳纳米材料具有良好的循环稳定性能和电化学电容特性。
(3)采用强氧化-声化学切割法制备出径向长度为10-300nm、两端开口的多壁富勒烯管，并将其与石墨烯构建出复合纳米膜材料。采用扫描电子显微电镜、N2吸脱附曲线和X射线衍射光谱研究了复合膜的形貌和结构，结果表明，富勒烯管可视为一种大分子化合物用以修饰石墨烯形成多孔三维膜结构的纳米复合材料。采用循环伏安和电化学阻抗谱研究了复合膜的电化学活性，结果表明，富勒烯管的引进有效地抑制了石墨烯的团聚，促进了电子或离子在电极材料的传递速率，提高了碳纳米管管体积的利用率，因此复合膜材料呈现出很高的电化学活性。该结果为促进碳纳米管在储能方面的应用提供了有力的依据。
(4)采用具有芳香烃大分子的中间相沥青为碳源，SBA~(-1)5型有序介孔硅为模板，通过模板碳化法制备出具有纳米石墨烯片孔壁结构的多孔碳材料，探讨了该材料的形成过程和研究了其锂离子电池负极性能。采用透射电子显微电镜、N2吸脱附曲线和X射线衍射光谱等研究了多孔碳的形貌和结构。结果表明，多孔碳材料具有二维有序且对称的六边形孔结构，孔壁由纳米石墨烯片层沿垂直于孔壁轴向定向堆积而成的。经50次循环充放电后，其i0和DLi值基本保持不变，甚至在高达3500mA g~(-1)电流密度下，其可逆比容量仍具有153.9mAh g~(-1)，展现出突出的倍率性能和优异的循环稳定性能。这些优异的锂离子负极性能主要取决于多孔碳材料具有多孔性的结构和纳米石墨烯片的孔壁结构。
(5)系统探讨了热处理温度对一步浸渍-模板碳化法制备的纳米石墨烯片堆积结构多孔碳材料的锂离子电池负极性能的影响。结果表明，在1200°C (C~(-1)200)的热处理温度下制备的多孔碳材料具有纳米石墨烯片状结构的孔壁，其可逆比容量为372mAh g~(-1)；随着热处理温度的升高，达到1800°C (C~(-1)800)时，多孔碳的纳米石墨烯片状结构越清晰，锂离子电池的比容量逐渐降低，然而功率性能却与C~(-1)200相似。但是在2400°C (C-2400)的热处理温度下，多孔碳发生了重排，其孔隙壁表现为成束的无孔纳米纤维结构，表现出低的比能量-比功率性能。由此可知，热处理温度由于能影响多孔碳材料的纳米石墨烯片孔壁结构，进而能影响该材料的锂离子电池负极性能。
Graphene, a single layer of carbon atoms with two-dimensional crystal structures,is a new member of the carbon family. Graphene has attracted great attention for itsoutstanding physical and chemical properties such as high specific surface area,conductivity, thermal stability and quantum tunnel effect. In the past decade, it hasbecome a research focus. The performance of carbon nanomaterial usually depends onits structure and morphology, which show great application potential in energy storage,catalysis, sensors and electronics, optics, etc. The main targets of this paper are asfollows:(1) Graphene is modified by physicochemical methods to obtaingraphene-based nanomaterials with more excellent performances;(2) the internalconnection of structures and electrochemical properties and the electrochemicalapplications (supercapacitors and lithium ion batteries) of graphene-basednanomaterials are systematically researched, which could lay the foundation ofpractical application of graphene nanomaterials. Main research contents are as follows:
(1) High-quality graphene scrolls (GSS) are designed using a facile and novelmicroexplosion method under an ultrasonic reaction between MnO2and H2O2. Themethodology successfully realizes the transformation from2-dimensional (2D)material to nearly1D material. The scrolled mechanism is proposed and theircapacitance properties are investigated in this work. Compared with the specificcapacity of110F g~(-1)for graphene sheets, a remarkable capacity of162.2F g~(-1)isobtained at the current density of1.0A g~(-1)in6M KOH aqueous solution due to theirunique scrolled conformation, porous structure, open ends/edges and adjustableinterlayer distance. The capacity value is increased by about50%only because of thetopological change of graphene sheets. Meanwhile, GSS exhibit excellent long-termcycling stability along with96.8%retained after1000cycles at1.0A g~(-1). All datassuggest that this study could offer an insightful approach for the preparation anddevelopment of GSS. These encouraging results indicate that GSS based on thetopological structure of graphene sheets are a kind of promising material forsupercapacitors.
(2) Partial scrolled graphene are designed by a simple microexplosion techniqueusing a mild ionic catalyst-Fe~(3+), and assemble sroll-sheet conjoined nanomaterials(GS-GSS) based on graphene (GS) with unscrolled parts for enhanced supercapacitor properties. The morphology and structure of GS-GSS are characterized bytransmmision electron microscope, N2adsorption/desorption, Raman spectra andenergy dispersive spectrometer. The results demonstrate that the scrolled structurepresents on the edges of GS form GS-GSS and the scroll rate of nanomaterials is about30%. Electrochemical dates show that the specific capacitance of GS-GSS (224F g~(-1)at1.0A g~(-1)in1M H2SO4) is much higher than that of GS (137F g~(-1)) andGS-MWCNTs-7-3(121F g~(-1)), the capacity value is increased by about100%onlybecause of the difference of tubular structure (scroll has the open ends and edges,while the carbon nanotubes are closed). Therefore, the GS-GSS are promisinggraphene-based materials for supercapacitors. What's more, it is expected for GS-GSSnanomaterials to replace the traditional GS-MWCNTs nanocomposites for potentialapplications in future.
(3) In this study, for increasing the utilization of closed pore volumes of carbonnanotubes (CNTs) in conventional graphene-CNTs composites, multi-wall fullerenenanopipes (MWFNs) are adopted to replace the pristine, nearly endless and highlytangled CNTs. The CNTs are tailored into MWFNs with10-300nm lengths and openends, and a nanocomposite film of well-dispersed MWFNs as macromolecules ongraphene (GS) is prepared by a facile wet-chemical route. The morphology of theresulting materials is characterized by scanning electron microscope (SEM) and theirelectrochemical activities are investigated, suggesting that the MWFNs asmacromolecules could uniformly modify and distribute on the surface of graphene andform a film structure with graphene. The introduction of MWFNs could effectivelyenhance the utilization of closed pore volumes of nanopipes, inhibit the stacking ofgraphene and facilitate the transportation of the electrolyte ion and electron in theelectrode. Such the GS/MWFNs nanocomposites obtain ultrahigh electrochemicalactivities. These results indicate that the unique MWFNs would stimulate thedevelopment of several energy-efficient technologies.
(4) An ordered mesoporous carbon (OMC) with controllable molecule crystal andplatelet graphitic pore walls, which is directionally grown on the internal pore walls ofSBA~(-1)5or anchors at liquid/silica interfaces by molecule engineering, has beeninvestigated as lithium ion anodes. It is found that the OMC exhibits high kinetics, rateand cycling performance. The i0and DLiare almost constant after50cycles. OMCshows a high reversible specific capacity of153.9mAh g~(-1)at the current density ashigh as3500mA g~(-1). The excellent electrochemical performance could be attributed tothe presence of the porosity and platelet graphitic pore walls.
(5) Mesoporous carbons (MCs) with nanosheet-like walls have been prepared aselectrodes for lithium-ion batteries by a simple one-step infiltrating method under theaction of capillary flow. The influence of heat treatment temperature on the surfacetopography, pore/phase structure and anode performances of as-prepared materials hasbeen investigated. The results reveal that melted liquid-crystal polycyclic aromatichydrocarbons could be anchored on liquid/silica interfaces by molecule engineering.After carbonization, the nanosheets are formed as the pore walls of MCs and areperpendicular to the long axis of pores. The anode properties demonstrate that C~(-1)200displays higher reversible capacitance than those treated in higher temperature. Therate performances of C~(-1)200and C~(-1)800are similar and more excellent than that ofC-2400. These improved lithium ion anode properties could be attributed to thenanosheet-like walls of MCs which can be influenced by the heat treatmenttemperature.
引文
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